Ethyl 6-methyl-5-nitrobenzo[b]thiophene-2-carboxylate synthesis
- Product Name:Ethyl 6-methyl-5-nitrobenzo[b]thiophene-2-carboxylate
- CAS Number:159730-73-1
- Molecular formula:C12H11NO4S
- Molecular Weight:265.29
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Yield:159730-73-1 99.8%
Reaction Conditions:
with sodium in ethanol; for 3 h;Inert atmosphere;Reflux;
Steps:
3.2 Step 2) 6 - methyl -5 - [b] thiophene nitrobenzene and -2 - carboxylic acid ethyl ester
In the 100 ml double-mouth bottle is added in ethanol (40 ml), under the protection of nitrogen by adding sodium metal (0.25 g, 11 mmol), stirring 20 minutes, in 5 °C adding mercapto ethyl acetate (1.21 ml, 11.0 mmol), continuing to stir 30 minutes after adding 2 - bromo -4 - methyl -5 - nitrobenzaldehyde (2.70 g, 11.1 mmol), then heating to reflux the reaction 3 hours. Cooling to room temperature, steams solvent, to the residue is added in dichloromethane (100 ml), followed by water (100 ml) and saturated salt water (100 ml) washing, dried with anhydrous sodium sulfate. Filtering, steams solvent, vacuum drying to obtain a pale yellow solid (2.93 g, 99.8%).
References:
CN109721536,2019,A Location in patent:Paragraph 0207; 0211; 0212
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